Development and validation of a SPE-UHPLC-fluorescence method for the analysis of ochratoxin-a in certain Turkish wines

Authors

DOI:

https://doi.org/10.20450/mjcce.2019.1624

Keywords:

UHPLC-FLD, ochratoxin A, Turkish wine, validation, SPE

Abstract

A sensitive Ultra-High Performance Liquid Chromatography (UHPLC)-fluorescence method was developed and validated for the determination of ochratoxin-A (OTA) in Turkish wine samples. Naphthalene was used as an internal standard in this study. OTA was separated on a C18 (3.0 mm × 100 mm × 1.8 µm) column and analyses were run under isocratic conditions, with a mobile phase consisting of water/acetonitrile/acetic acid (50:50:1, v/v/v). The flow rate and injection volume were 0.5 ml min−1 and 10 μl, respectively. The excitation and emission wavelengths were 330 nm and 460 nm for OTA, respectively, and 220 nm and 325 nm for internal standard, respectively. A solid-phase extraction (SPE) clean-up procedure on a C18 cartridge was used prior to the analysis of the wine samples by UHPLC. The developed method was validated with respect to linearity, precision, accuracy, limit of detection (LOD), limit of quantitation (LOQ), stability and robustness. The method presented good RSD (< 4 %) and recovery (102.6–105.2 %) values. The LOD and LOQ values were 0.01 ng ml1 and 0.05 ng ml1, respectively. All other parameters were acceptable. OTA amounts were found in the range of 2.72‒7.40 µg kg‒1 in the Turkish wine samples.

References

M. E. Zain, Impact of mycotoxins on humans and animals, J. Saudi Chem. Soc. 15, 129–144 (2011).

DOI: https://doi.org/10.1016/j.jscs.2010.06.006

A. Visconti, M. Pascale, G. Centonze, Determination of ochratoxin A in wine by means of immunoaffinity column clean-up and high-performance liquid chro-matography, J. Chromatogr. A 864, 89–101 (1999).

DOI: https://doi.org/10.1016/S0021-9673(99)00996-6

E. Anlı, M. Bayram; Ochratoxin A in wines, Food Rev. Int. 25, 214–232 (2009).

DOI: http://dx.doi.org/10.1080/87559120902956182

V. Ostrý, F. Malir, M. Dofková, J. Skarková, A. Pfohl-Leszkowicz, J. Ruprich, Ochratoxin A dietary expo-sure of ten population groups in the Czech Republic: comparison with data over the world, Toxins 7, 3608–3635 (2015). DOI: 10.3390/toxins7093608

A. Khoury, A. Atoui, Ochratoxin A: General overview and actual molecular status, Toxins 2, 461–493 (2010). DOI: 10.3390/toxins2040461

F. J. Cabanes, F. Accensi, M. R. Bragulat, M. L. Abar-ca, G. Castella, S. Minguez, A. Pons, What is the source of ochratoxin A in wine?, Int. J. Food Micro-biol. 79, 213–215, (2002).

DOI: https://doi.org/10.1016/S0168-1605(02)00087-9

I. Var, B. Kabak, Occurrence of ochratoxin A in Turk-ish Wines, Microchem. J. 86(2), 241–247 (2007).

DOI: 10.1016/j.microc.2007.04.002

FAO/WHO (Food and Agriculture Organisation/World Health Organisation), Ochratoxin A. In: Safety evalua-tion of certain mycotoxins in food, Prepared by the 56th Meeting of the Joint FAO/WHO Expert Commit-tee on Food Additives (JECFA). WHO Food Additives Series 47, Geneva, Switzerland, 2001, 281–387.

EC (European Community), Opinion of the Scientific Committee on Food (SCF) on Ochratoxin A, 1998.

Commission Regulation (EC) 1881/2006, Setting Max-imum Levels for Certain Contaminants in Foodstuffs, Off J. Eur. Union L. 364, 5–24 (2006).

A. G. Frenich, R. Romero-González, M. M. Aguilera-Luiz, Comprehensive analysis of toxics (pesticides, veterinary drugs and mycotoxins) in food by UHPLC-MS, Trends Anal. Chem. 63, 158–169 (2014).

DOI: http://dx.doi.org/10.1016/j.trac.2014.06.020

I. Barna-Vetro, L. Solti, J. Teren, E. Gyongsyösi, E. Szabo, A. Wölfling, Sensitive ELISA test for determi-nation of ochratoxin A, J. Agric. Food Chem. 44, 4071–4074, (1996). DOI: 10.1021/jf960442n

Z. Zheng, J. Hanneken, D. Houchins, R. S. King, P. Lee, J. L. Richard, Validation of an ELISA test kit for the detection of ochratoxin A in several food com-modities by comparison with HPLC, Mycopathologia 159, 265–272 (2005). DOI: 10.1007/s11046-004-8663-3

A. Pittet, D. Royer, Rapid, low cost thin-layer chroma-tographic screening method for the detection of ochra-toxin A in green coffee at a control level of 10 µg/kg, J. Agric. Food Chem. 50, 243–247 (2002).

DOI: 10.1021/jf010867w

Y. Jiao, W. Blaas, C. Rühl, R. Weber, Identification of ochratoxin A in food samples by chemical derivatiza-tion and gas chromatography-mass spectrometry, J. Chromatogr. A 595, 364–367 (1992).

DOI: 10.1016/0021-9673(92)85183-T

J. Olsson, T. Borjesson, T. Lundstedt, J. Schnurer, Detection and quantification of ochratoxin A and de-oxynivalenol in barley grains by GC-MS and electron-ic nose, Int. J. Food Microbiol. 72, 203–214 (2002).

DOI: https://doi.org/10.1016/S0168-1605(01)00685-7

H. Y. Aboul-Enein, Ö. B. Kutluk, G. Altiokka, M. Tunçel, A modified HPLC method for the determina-tion of ochratoxin A by fluorescence detection, Bio-med. Chromatogr. 16, 470–474 (2002).

DOI: 10.1002/bmc.187

J. Skarkova, V. Ostry, F. Malir, T. Roubal, Determina-tion of ochratoxin A in food by high performance liq-uid chromatography, Anal. Lett. 46, 1495–1504 (2013). DOI: 10.1080/00032719.2013.771266

M. Ibáñez-Vea, L. A. Corcuera, R. Remiro, M. T. Mu-rillo-Arbizu, E. González-Peñas, E. Lizarraga, Valida-tion of a UHPLC-FLD method for the simultaneous quantification of aflatoxins, ochratoxin A and zeara-lenone in barley, Food Chem. 127, 351–358 (2011).

DOI: 10.1016/j.foodchem.2010.12.157

M. Mincea, C. Ionascu, K. Kis, V. Ostafe, Detection of ochratoxin A in instant coffee by UPLC-MS/MS, Studia UBB Chemia 2, 167–175 (2016).

M. W. Dong, K. Zhang, Ultra-High-Pressure liquid chromatography (UHPLC) in method development, Trends Analyt. Chem. 63, 21–30 (2014).

DOI: 10.1016/j.trac.2014.06.019

S. Fekete, J. Schappler, J.-L. Veuthey, D. Guillarme, Current and future trends in UHPLC, Trends Analyt. Chem. 63, 2–13 (2014).

DOI: 10.1016/j.trac.2014.08.007

I. Klimczak, A. Gliszczynska-Swigło, Comparison of UPLC and HPLC methods for determination of vita-min C, Food Chem. 175, 100–105 (2015).

DOI: 10.1016/j.foodchem.2014.11.104

R. Mikulíková, S. Beláková, K. Benešová, Z. Svo-boda, Study of ochratoxin A content in South Moravi-an and foreign wines by the UPLC method with fluo-rescence detection, Food Chem. 133, 55–59 (2012).

DOI: 10.1016/j.foodchem.2011.12.061

C. L. De Jesus, A. Bartley, A. Z. Welch, J. P. Berry, High incidence and levels of ochratoxin A in wines sourced from the United States, Toxins 10, 1–12 (2018). DOI: 10.3390/toxins10010001

F. Gentile, G. L. La Torre, A. G. Potortì, M. Saitta, M. Alfa, G. Dugo, Organic wine safety: UPLC-FLD de-termination of ochratoxin A in Southern Italy wines from organic farming and winemaking, Food Control 59, 20–26 (2016). DOI: 10.1016/j.foodcont.2015.05.006

J. Li, X. Liu, S. Han, J. Li, Q. Xu, H. Xu, Y. Wang, F. Liu, Z. Zhang, Analysis of ochratoxin A in wine by High-Resolution UHPLC-MS, Food Anal. Methods 5, 1506–1513 (2012).

DOI: https://doi.org/10.1007/s12161-012-9403-9

A. Leitner, P. Zöllner, A. Paolillo, J. Stroka, A. Papa-dopoulou-Bouraoui, S. Jaborek, E. Anklam, W. Lind-ner, Comparison of methods for the determination of ochratoxin A in wine, Anal. Chim. Acta 453, 33–41 (2002). DOI: 10.1016/S0003-2670(01)01483-0

E. Anlı, B. Çabuk, N. Vural, E. Başpınar, Ochratoxin A in Turkish wines, J. Food Biochem. 29, 611–623 (2005). DOI: https://doi.org/10.1111/j.1745-4514.2005.00043.x

G. Altiokka, N. O. Can, Z. Atkoşar, H. Y. Aboul-Enein, Determination of ochratoxin A in Turkish wines, JFDA 17(6), 467–473 (2009).

M. J. Hernandez, M. V. Garcia-Moreno, E. Duran, D. Guillen, C. G. Barroso, Validation of two analytical methods for the determination of ochratoxin A by re-versed-phased High-Performance Liquid Chromatog-raphy coupled to fluorescence detection in musts and sweet wines from Andalusia, Anal. Chim. Acta 566, 117–121 (2006). DOI: 10.1016/j.aca.2006.02.002

The International Conference on Harmonization (ICH), Validation of Analytical Procedures: Method-ology, Topic Q2B, CPMP/ICH/281/95, 1996.

N. Belli, S. Marin, V. Sanchis, A. J. Ramos, Review: Ochratoxin A (OTA) in wines, musts and grape juices: Occurrence, regulations and methods of analysis, Food Sci. Tech. Int. 8(6), 325–335 (2002).

DOI: https://doi.org/10.1106/108201302031863

A.-M. Turcotte, P. M. Scott, Ochratoxin A in cocoa and chocolate sampled in Canada, Food Addit. Con-tam. 28, 762–766 (2011). DOI: 10.1080/19440049.2010.508796

L. Campone, A. L. Piccinelli, L. Rastrelli, Dispersive liquid–liquid microextraction combined with high-performance liquid chromatography–tandem mass spectrometry for the identification and the accurate quantification by isotope dilution assay of Ochratoxin A in wine samples, Anal. Bioanal. Chem. 399, 1279–1286 (2011). DOI: https://doi.org/10.1007/s00216-010-4347-7

D. Jornet, O. Busto, J. Guasch, Solid-phase extraction applied to the determination of ochratoxin A in wines by reversed-phase high-performance liquid chroma-tography, J. Chromatogr. A 882, 29–35 (2000).

DOI: https://doi.org/10.1016/S0021-9673(00)00237-5

J. M. Sáez, Á. Medina, J. V. Gimeno-Adelantado, R. Mateo, M. Jiménez, Comparison of different sample treatments for the analysis of ochratoxin A in must, wine and beer by liquid chromatography, J. Chroma-togr. A 1029, 125–133 (2004).

DOI: https://doi.org/10.1016/j.chroma.2003.12.021

A. Prelle, D. Spadaro, A. Denca, A. Garibaldi, M. L. Gullino, Comparison of clean-up methods for ochra-toxin A on wine, beer, roasted coffee and chili com-mercialized in Italy, Toxins 5, 1827–1844 (2013).

DOI: https://doi.org/10.3390/toxins5101827

A.-M. Nistor, S.-D. Cotan, C.-B. Nechita, A. Tartian, M. Niculaua, V. V. Cotea, Rapid assessment of myco-toxins in wine by on-line SPE-UHPLC-FLD, BIO Web of Conferences 9, 6 (2017).

DOI: https://doi.org/10.1051/bioconf/20170902022

Commission Regulation (EC) No 401/2006 of 23 Feb-ruary 2006 Laying Down the Methods of Sampling and Analysis for the Official Control of the Levels of Mycotoxins in Foodstuffs, Off. J. Eur. Union L70, 12–34 (2006).

Commission Regulation (EC) No 519/2014 of 16 May 2014 amending Regulation (EC) No 401/2006 As Re-gards Methods of Sampling of Large Lots, Spices and Food Supplements, Performance Criteria for T-2, HT-2 Toxin and Citrinin and Screening Methods of Analy-sis. Off. J. Eur. Union L147, 29–43 (2014).

Downloads

Published

2019-12-30

How to Cite

Oncu Kaya, E. M. (2019). Development and validation of a SPE-UHPLC-fluorescence method for the analysis of ochratoxin-a in certain Turkish wines. Macedonian Journal of Chemistry and Chemical Engineering, 38(2), 161–170. https://doi.org/10.20450/mjcce.2019.1624

Issue

Section

Analytical Chemistry